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Triethylamine → HCID 71226964, compound

HRID 2359368
Notes
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Reaction equation

HRID 2359368 reaction equation
Cl.[CH2:2]1[C:5]2([CH2:9][CH2:8][CH2:7][O:6]2)[CH2:4][NH:3]1.C(N(CC)CC)C.[CH3:17][O:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]2[O:29][C:28]([C:30]([N:32]3[CH2:35][CH:34]([O:36][C:37]4[CH:44]=[CH:43][C:40]([CH:41]=O)=[CH:39][CH:38]=4)[CH2:33]3)=[O:31])=[N:27][N:26]=2)=[CH:21][CH:20]=1.[Na].C([O-])(O)=O.[Na+]>ClCCl>[CH2:4]1[C:5]2([CH2:9][CH2:8][CH2:7][O:6]2)[CH2:2][N:3]1[CH2:41][C:40]1[CH:39]=[CH:38][C:37]([O:36][CH:34]2[CH2:35][N:32]([C:30]([C:28]3[O:29][C:25]([C:22]4[CH:23]=[CH:24][C:19]([O:18][CH3:17])=[CH:20][CH:21]=4)=[N:26][N:27]=3)=[O:31])[CH2:33]2)=[CH:44][CH:43]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 5360545SodiumHCID 580430894-(1-(5-(4-Methoxyphenyl)-1,3,4-oxadiazole-2-carbonyl)azetidin-3-yloxy)benzaldehydeHCID 862803555-Oxa-2-azaspiro[3.4]octane hydrochloride

Product 1

HCID 71226964
HCID 71226964, compound
Yield 17%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

5-Oxa-2-azaspiro[3.4]octane HCl salt (0.052 g, 0.35 mmol) was dissolved in dichloromethane (2 ml). Triethylamine (0.052 ml, 0.38 mmol) was added, followed by 4-(1-(5-(4-methoxyphenyl)-1,3,4-oxadiazole-2-carbonyl)azetidin-3-yloxy)benzaldehyde (0.11 g, 0.29 mmol) and finally sodium triacetoxyhydroborate (0.123 g, 0.58 mmol). The reaction was stirred at ambient temperature overnight. The reaction mixture was then diluted with dichloromethane (10 ml) and subsequently shaken with NaHCO3 (sat. 2 ml). The two phases were separated using a phase separator. The organic phase was evaporated. The product was purified by preparative reverse-phase HPLC at pH 10 to give 23 mg (17%) of the desired product as a solid. 1H NMR (500 MHz, CDCl3): δ 1.90 (p, 2H), 2.13 (t, 2H), 3.16 (d, 2H), 3.37 (d, 2H), 3.62 (s, 2H), 3.80 (t, 2H), 3.91 (s, 3H), 4.33 (dd, 1H), 4.62-4.7 (m, 1H), 4.73-4.78 (m, 1H), 5.03-5.16 (m, 2H), 6.74 (d, 2H), 7.04 (d, 2H), 7.25 (d, 2H), 8.11 (d, 2H). MS (APCI+) m/z 477.3 [M+H]+, LC purity: 97%

Workup

  1. customThe two phases were separated
  2. customThe organic phase was evaporated
  3. customThe product was purified by preparative reverse-phase HPLC at pH 10

Sources & evidence

ORD record
ord-2c153e7d134448e8aee91470728745bd
Source dataset
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08685958B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes